CN104004515B - A kind of preparation method of strontium aluminate long-afterglow luminescent materials - Google Patents
A kind of preparation method of strontium aluminate long-afterglow luminescent materials Download PDFInfo
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- CN104004515B CN104004515B CN201410269243.5A CN201410269243A CN104004515B CN 104004515 B CN104004515 B CN 104004515B CN 201410269243 A CN201410269243 A CN 201410269243A CN 104004515 B CN104004515 B CN 104004515B
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Abstract
The present invention discloses a kind of preparation method of strontium aluminate long-afterglow luminescent materials, comprises the steps: that the nitrate of aluminum nitrate and strontium or carbonate distilled water dissolve by (1) and obtains solution, add boric acid and swelling agent; (2) in the mixture of europium sesquioxide and dysprosium oxide, nitric acid is added; (3) the two kinds of solution mixing obtained in step (1), (2), add surface-modifying agent, ageing 10min ~ 5h; (4) mixing solutions obtained for step (3) is loaded crucible, put into the retort furnace of 350 ~ 450 DEG C, be warming up to 500 ~ 600 DEG C, temperature rise rate 5 DEG C/min, insulation 20min, then be warming up to 900 ~ 1500 DEG C, temperature rise rate is 10 ~ 20 DEG C/min, insulation 20min ~ 3h.The invention solves the hard aggregation problem that conventional sintering method occurs, owing to adopting raising agent to make the luminescent material outward appearance of synthesis be spumescence loosening body, very easily levigate, do not affect the luminosity of product.
Description
Technical field
The present invention relates to a kind of preparation method of strontium aluminate long-afterglow luminescent materials.
Background technology
Rare-earth ion activated strontium aluminate (SrAl
2o
4: Eu
2+, Dy
3+) to have luminosity high for system energy-saving luminous material, time of persistence is long, not containing advantages such as radioelement, is widely used in the fields such as building, boats and ships, instrument, coatings industry, ink, glaze, plastics.At present, prepare strontium aluminate luminous material and mainly contain high temperature solid-phase sintering method, coprecipitation method, sol-gel and combustion method.Such as, Chinese technological invention patent CN 1188788, CN 1445330 A, CN 1699506 A, CN 1403533A etc. disclose and adopt solid phase method high temperature sintering to obtain luminescent material.China technological invention patent CN1389541A, CN 1563171 A report the technique adopting coprecipitation method to prepare luminescent material.Chinese patent CN 1401731 A, CN 1159411C, CN 1197831 A utilize sol-gel method and CN 1632053 A to adopt combustion method to prepare long-afterglow luminous alaminate powder.
All there is following weak point in above preparation technology: (1) flow process is complicated, needs the techniques such as batching, mixing, drying, sintering, fine grinding, causes the production cycle long.(2) the luminescent material hard aggregation prepared by is more severe, especially solid phase high-temperature sintering process, and sintered particles hardness, up to Mohs 6-7 level, is unfavorable for grinding and processing, directly causes particle thick, and in pulverizing and jevigating process, cause powder brightness to reduce; (3) reducing gas (CO or H is adopted
2), make production operation security bad.
Except existing problems in above-mentioned technique, prepared luminescent powder also existing defects in application performance.Wherein distinct issues are that aluminium strontium salt luminescent material facile hydrolysis in water generates aluminium hydroxide white precipitate the most, thus luminous intensity is sharply declined until completely lose luminous power, affect work-ing life.In addition, because the density of inorganic materials is large, with organism poor compatibility, be easily separated between luminescent powder and organic phase or macromolecular material, formation precipitates, and has a strong impact on material property.These problems all limit the application of luminescent material, the application especially in high-grade ink and the field such as paint and textile printing and dyeing.
Summary of the invention
Goal of the invention: the object of the invention is for the deficiencies in the prior art, there is provided a kind of preparation method with the strontium aluminate long-afterglow luminescent materials of lipophilicity and high-specific surface area, to solve the problems such as the particle thick, facile hydrolysis, the poor compatibility that exist when alumine acid strontium long afterglow luminescent powder is applied in ink, paint, field of textiles.
Technical scheme: the preparation method of strontium aluminate long-afterglow luminescent materials of the present invention, comprises the steps:
(1) nitrate of aluminum nitrate and strontium or carbonate distilled water are dissolved obtain solution, then add boric acid and swelling agent in the solution, mix;
(2) in the mixture of europium sesquioxide and dysprosium oxide, add nitric acid, regulate pH to be 5 ~ 6, be heated to temperature and be 60 ~ 80 DEG C and all dissolve to mixture;
(3) two kinds of solution mixing step (1) and step (2) obtained, add surface-modifying agent, at 60 ~ 80 DEG C of ageing 10min ~ 5h;
(4) mixing solutions obtained for step (3) is loaded crucible, put into the retort furnace of 350 ~ 450 DEG C, be warming up to 500 ~ 600 DEG C, temperature rise rate 5 ~ 10 DEG C/min, insulation 15 ~ 30 min, then be warming up to 900 ~ 1500 DEG C, temperature rise rate is 10 ~ 20 DEG C/min, is incubated 20 min ~ 3h; Finally be cooled to room temperature and obtain described strontium aluminate long-afterglow luminescent materials
Preferably, in solution, the volumetric molar concentration of strontium element is 0.15 ~ 0.3M, and the mol ratio of strontium and aluminium element is 1:1.9 ~ 2.1; Further preferably, in solution, the volumetric molar concentration of strontium element is 0.2M, and the mol ratio of strontium and aluminium element is 1:2.
Preferably, in step (1), the mol ratio of strontium element and boric acid is 1:0.3 ~ 0.5, and the mol ratio of strontium element and swelling agent is 1:2 ~ 5; Further preferably, the mol ratio of strontium element and boric acid is 1:0.3, and the mol ratio of strontium element and swelling agent is 1:3.
Preferably, described swelling agent is one or more in oxalic acid, tartrate, citric acid, glucose, urea.
Preferably, in step (2), the mol ratio of europium and dysprosium element is 1:1 ~ 2, and the volumetric molar concentration of nitric acid is 0.1 ~ 0.3M; Further preferably, in step (2), the mol ratio of europium and dysprosium element is 1:2, and the volumetric molar concentration of nitric acid is 0.1M.
Preferably, in step (3), two kinds of solution mixing that step (1) and step (2) are obtained, mol ratio=1:0.012 ~ 0.013 of Sr:Eu after mixing.
Preferably, in step (3), the consumption of surface-modifying agent is 0.2 ~ 5% of mixing solutions gross weight.
Preferably, in step (3), described surface-modifying agent is TiO
2or/and SiO
2nano particle, the diameter of particle is 2 ~ 10 nm.
Preferably, in step (4), mixing solutions is loaded crucible, put into the retort furnace of 400 DEG C, be warming up to 600 DEG C from 400 DEG C, temperature rise rate 5 DEG C/min, is incubated 20 min, then is warming up to 1000 DEG C, and temperature rise rate is 10 DEG C/min, insulation 1h; Finally be cooled to room temperature and obtain described strontium aluminate long-afterglow luminescent materials.
Beneficial effect: the product that the inventive method obtains can be widely used in the field such as luminescent plastics, luminous paint, luminous printing ink, luminous paint that organism or polymer are matrix, be used for making various luminous sign, light-emitting workmanship, optoelectronic device and display material etc., compared with prior art, the product that prepared by the inventive method has following features:
(1) the hard aggregation problem that conventional sintering method occurs is solved, owing to adopting raising agent to make the luminescent material outward appearance of synthesis be spumescence loosening body, very easily levigate, do not affect the luminosity of product;
(2) the inventive method is owing to adopting liquid phase synthesizing method, and prepared luminescent powder particle is thinner, particle diameter evenly, cause high specific surface, without problems such as incandescnet particle dead layers, finally cause usage quantity in the application significantly to reduce;
(3) surface-modifying agent added in the inventive method makes the resistant to hydrolysis characteristic of product and consistency significantly be improved, while the dispersion effect improving powder, also help the diffusion of luminescent center ion, and can also the effect of effectively playing Trapping Centers the same as common doped with rare earth ion, thus extend time of persistence, strengthen illumination effect;
(4) the inventive method technique is simple, with short production cycle, is convenient to use of large-scale production.
Embodiment
Below technical solution of the present invention is described in detail, but protection scope of the present invention is not limited to described embodiment.
embodiment 1:a preparation method for strontium aluminate long-afterglow luminescent materials, comprises the steps:
(1) take 18g nine water aluminum nitrate and 5g anhydrous strontium nitrate, dissolve with 100 ml distilled water, add 0.3g boric acid, add 46g urea as swelling agent, Homogeneous phase mixing.
(2) take 0.05g europium sesquioxide and 0.05g dysprosium oxide, add the nitric acid dissolve of 0.1M, pH=5 ~ 6 in mixture, 60 ~ 80 DEG C of insulation to mixtures all dissolve.
(3) by above-mentioned two kinds of solution mixing, 1.1g nano-TiO is added
2, 60 ~ 80 DEG C of ageing 10 min.
(4) mixed solution loads the retort furnace that crucible puts into 400 DEG C.Be warming up to 600 DEG C from 400 DEG C, temperature rise rate 5 DEG C/min, is incubated 20 min, then is warming up to 900 DEG C, and temperature rise rate is 10 DEG C/min, is incubated 20 min.Be cooled to room temperature, sampling.Namely alumine acid strontium long afterglow high-brightness luminous material of the present invention is obtained.
Luminescent material outward appearance prepared by this embodiment is light green, and powder median size is 200 nm.Well excite in visible-range, glow peak wavelength is 520 nm, and illuminant colour is green, and original intensity reaches 17500 mcd/m
2, time of persistence can know (0.32mcd/m in brightness range at human eye
2) be greater than 8 hours.
embodiment 2:a preparation method for strontium aluminate long-afterglow luminescent materials, comprises the steps:
(1) take 18g nine water aluminum nitrate and 5g anhydrous strontium nitrate, dissolve with 20 ml distilled water, add 0.3g boric acid, add 2.3g oxalic acid as swelling agent, Homogeneous phase mixing.
(2) take 0.05g europium sesquioxide and 0.05g dysprosium oxide, add the nitric acid dissolve of 0.1M, pH=5 ~ 6 in mixture, 60 ~ 80 DEG C of insulation to mixtures all dissolve.
(3) by above-mentioned two kinds of solution mixing, 0.05g Nano-meter SiO_2 is added
2, 60 ~ 80 DEG C of ageing 5h.
(4) mixed solution loads the retort furnace that crucible puts into 350 DEG C.Be warming up to 600 DEG C from 350 DEG C, temperature rise rate 5 DEG C/min, is incubated 20 min, then is warming up to 1500 DEG C, and temperature rise rate is 10 DEG C/min, insulation 3h.Be cooled to room temperature, sampling.Namely alumine acid strontium long afterglow high-brightness luminous material of the present invention is obtained.
Luminescent material outward appearance prepared by this embodiment is light green, and powder median size is 90 nm.Well excite in visible-range, glow peak wavelength is 518 nm, and illuminant colour is yellow-green colour, and original intensity reaches 18500 mcd/m
2, time of persistence can know (0.32mcd/m in brightness range at human eye
2) be greater than 8 hours.
embodiment 3:a preparation method for strontium aluminate long-afterglow luminescent materials, comprises the steps:
(1) take 18g nine water aluminum nitrate and 5g anhydrous strontium nitrate, dissolve with 100 ml distilled water, add 0.3g boric acid, add 10g oxalic acid and 10g citric acid as swelling agent, Homogeneous phase mixing.
(2) take 0.05g europium sesquioxide and 0.05g dysprosium oxide, in mixture, add the nitric acid dissolve of 0.1M, pH=5 ~ 6,60 ~ 80 DEG C of insulations.
(3) by above-mentioned two kinds of solution mixing, 0.2g Nano-meter SiO_2 is added
2with 0.6g nano-TiO
2, 60 ~ 80 DEG C of ageing 2h.
(4) mixed solution loads the retort furnace that crucible puts into 450 DEG C.Be warming up to 500 DEG C from 450 DEG C, temperature rise rate 5 DEG C/min, is incubated 20 min, then is warming up to 1500 DEG C, and temperature rise rate is 10 DEG C/min, insulation 1h.Be cooled to room temperature, sampling.Namely alumine acid strontium long afterglow high-brightness luminous material of the present invention is obtained.
Luminescent material outward appearance prepared by this embodiment is light green, and powder median size is 180 nm.Well excite in visible-range, glow peak wavelength is 518 nm, and illuminant colour is yellow-green colour, and original intensity reaches 18000 mcd/m
2, time of persistence can know (0.32mcd/m in brightness range at human eye
2) be greater than 8 hours.The oil number of luminescent material is 15 ml/100g, and the luminescent material oil number do not added prepared by raising agent and surface-modifying agent is 32 ml/100g.
embodiment 4:a preparation method for strontium aluminate long-afterglow luminescent materials, comprises the steps:
(1) take 18g nine water aluminum nitrate and 3.49g Carbon Dioxide strontium, dissolve with 100 ml distilled water, add 0.3g boric acid, add 5g glucose as swelling agent, Homogeneous phase mixing.
(2) take 0.05g europium sesquioxide and 0.05g dysprosium oxide, in mixture, add the nitric acid dissolve of 0.1M, pH=5 ~ 6,60 ~ 80 DEG C of insulations.
(3) by above-mentioned two kinds of solution mixing, 0.4g Nano-meter SiO_2 is added
2, 60 ~ 80 DEG C of ageing 2h.
(4) mixed solution loads the retort furnace that crucible puts into 450 DEG C.Be warming up to 500 DEG C from 450 DEG C, temperature rise rate 5 DEG C/min, is incubated 20 min, then is warming up to 1500 DEG C, and temperature rise rate is 10 DEG C/min, insulation 1h.Be cooled to room temperature, sampling.Namely alumine acid strontium long afterglow high-brightness luminous material of the present invention is obtained.
Luminescent material outward appearance prepared by this embodiment is light green, and powder median size is 120 nm.Well excite in visible-range, glow peak wavelength is 518 nm, and illuminant colour is yellow-green colour, and original intensity reaches 19500 mcd/m
2, time of persistence can know (0.32mcd/m in brightness range at human eye
2) be greater than 8 hours.
As mentioned above, although represented with reference to specific preferred embodiment and described the present invention, it shall not be construed as the restriction to the present invention self.Under the spirit and scope of the present invention prerequisite not departing from claims definition, various change can be made in the form and details to it.
Claims (9)
1. a preparation method for strontium aluminate long-afterglow luminescent materials, is characterized in that comprising the steps:
(1) nitrate of aluminum nitrate and strontium or carbonate distilled water are dissolved obtain solution, then add boric acid and swelling agent in the solution, mix;
(2) in the mixture of europium sesquioxide and dysprosium oxide, add nitric acid, regulate pH to be 5 ~ 6, be heated to temperature and be 60 ~ 80 DEG C and all dissolve to mixture;
(3) two kinds of solution mixing step (1) and step (2) obtained, add surface-modifying agent, at 60 ~ 80 DEG C of ageing 10min ~ 5h; Described surface-modifying agent is TiO
2or/and SiO
2nano particle, the diameter of particle is 2 ~ 10 nm;
(4) mixing solutions obtained for step (3) is loaded crucible, put into the retort furnace of 350 ~ 450 DEG C, be warming up to 500 ~ 600 DEG C, temperature rise rate 5 ~ 10 DEG C/min, insulation 15 ~ 30 min, then be warming up to 900 ~ 1500 DEG C, temperature rise rate is 10 ~ 20 DEG C/min, is incubated 20 min ~ 3h; Finally be cooled to room temperature and obtain described strontium aluminate long-afterglow luminescent materials.
2. the preparation method of strontium aluminate long-afterglow luminescent materials according to claim 1, is characterized in that: in step (1), and in solution, the volumetric molar concentration of strontium element is 0.15 ~ 0.3M, and the mol ratio of strontium and aluminium element is 1:1.9 ~ 2.1.
3. the preparation method of strontium aluminate long-afterglow luminescent materials according to claim 1, is characterized in that: in step (1), and in solution, the volumetric molar concentration of strontium element is 0.2M, and the mol ratio of strontium and aluminium element is 1:2.
4. the preparation method of strontium aluminate long-afterglow luminescent materials according to claim 1, is characterized in that: in step (1), and the mol ratio of strontium element and boric acid is 1:0.3 ~ 0.5, and the mol ratio of strontium element and swelling agent is 1:2 ~ 5.
5. the preparation method of strontium aluminate long-afterglow luminescent materials according to claim 1, is characterized in that: described swelling agent is one or more in oxalic acid, tartrate, citric acid, glucose, urea.
6. the preparation method of strontium aluminate long-afterglow luminescent materials according to claim 1, is characterized in that: in step (2), and the mol ratio of europium and dysprosium element is 1:1 ~ 2, and the volumetric molar concentration of nitric acid is 0.1 ~ 0.3M.
7. the preparation method of strontium aluminate long-afterglow luminescent materials according to claim 1, is characterized in that: in step (3), two kinds of solution mixing step (1) and step (2) obtained, mol ratio=1:0.012 ~ 0.013 of Sr:Eu after mixing.
8. the preparation method of strontium aluminate long-afterglow luminescent materials according to claim 1, is characterized in that: in step (3), and the consumption of surface-modifying agent is 0.2 ~ 5% of mixing solutions gross weight.
9. the preparation method of strontium aluminate long-afterglow luminescent materials according to claim 1, it is characterized in that: in step (4), mixing solutions is loaded crucible, put into the retort furnace of 400 DEG C, be warming up to 600 DEG C from 400 DEG C, temperature rise rate 5 DEG C/min, be incubated 20 min, be warming up to 1000 DEG C again, temperature rise rate is 10 DEG C/min, insulation 1h; Finally be cooled to room temperature and obtain described strontium aluminate long-afterglow luminescent materials.
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| CN108010463A (en) * | 2017-12-12 | 2018-05-08 | 青岛伟健金属饰品有限公司 | A kind of light emitting directory board used preparation process of traffic |
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